Ethanolamine → 2-Chloro-6-(2-hydroxyethyl)-6,7-dihydro-5H-pyrrolo[3,4-b]pyridin-5-one

HRID 1799545노트

반응식

HRID 1799545 반응식
[Cl:1][C:2]1[N:7]=[C:6]([CH2:8]Cl)[C:5]([C:10]([O:12]C)=O)=[CH:4][CH:3]=1.[CH2:14]([CH2:16][NH2:17])[OH:15]>CO>[Cl:1][C:2]1[N:7]=[C:6]2[CH2:8][N:17]([CH2:16][CH2:14][OH:15])[C:10](=[O:12])[C:5]2=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 700Ethanolamine3회HCID 59525762Methyl 6-chloro-2-(chloromethyl)pyridine-3-carboxylate

생성물 1

HCID 582166462-Chloro-6-(2-hydroxyethyl)-6,7-dihydro-5H-pyrrolo[3,4-b]pyridin-5-one

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl 6-chloro-2-(chloromethyl)pyridine-3-carboxylate (0.1 g, 0.45 mmol) and ethanolamine (0.11 mL, 1.82 mmol) were stirred in MeOH (10 mL) at room temperature overnight. Additional ethanolamine (0.11 mL, 1.82 mmol) was added and stirring continued for 8 hours. Additional ethanolamine (0.22 mL, 3.64 mmol) was then added and stirring continued for 3 days. The solvent was removed in vacuo and the residue purified by silica gel chromatography (0-5% MeOH/EtOAc) to give the title compound as a white solid.

후처리

  1. stirringstirring
  2. waitcontinued for 3 days
  3. customThe solvent was removed in vacuo
  4. customthe residue purified by silica gel chromatography (0-5% MeOH/EtOAc)

출처 및 근거

ORD 기록
ord-87509003de184f31a930ef55e7722664
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08344144B2

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